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1.
高效液相色谱法测定河道底泥中的多环芳烃   总被引:1,自引:0,他引:1  
用高效液相色谱法分离测定河道底泥中的多环芳烃,通过梯度淋洗使多种多环芳烃完全分离,并分别得到14种多环芳烃的检出限和线性范围,被试验的4种多环芳烃的回收率为94.1%~103.1%,相对标准偏差为1.00%。2.87%(n=7)。用该方法对小清河东营段的实际底泥样品中多环芳烃的含量进行了测定。  相似文献   

2.
超临界流体萃取环境模拟样品中多环芳烃的收集方法研究   总被引:15,自引:0,他引:15  
 详细系统地研究了收集溶剂的种类、用量及无溶剂固体表面冷冻捕集等方法对离线收集超临界流体萃取多环芳烃组分效率的影响。研究发现,二氯甲烷和丙酮的收集效率较高,其回收率为61.44%~105.40%,其它有机溶剂效果较差。而且,当收集溶剂的液面高度大于2.0cm时,溶剂的用量对收集效率没有明显的影响。玻璃珠固体表面冷冻捕集效果较好,其回收率在60.98%~109.88%之间,但其精密度较差,相对标准偏差(RSD)在0.28%~11.29%之间。  相似文献   

3.
以二硫化碳为萃取剂,丙酮为分散剂对水样和土壤样中残留的多环芳烃进行分散液相微萃取。提取液供高效液相色谱仪的二极管阵列检测器和荧光检测器测定。选用LiChrospherPAH色谱柱作为固定相,用乙腈和水以不同比例混合的溶液作为流动相进行梯度淋洗。在优化的试验条件下,对合成水样中多环芳烃的富集倍数达220~560倍,16种多环芳烃可有效分离并测定。16种多环芳烃的检出限(3S/N)在0.002~0.05μg.L-1之间。用标准加入法测得回收率在64%~108%之间,测定值的相对标准偏差(n=7)在2.0%~7.8%之间。  相似文献   

4.
固相萃取搅拌棒萃取-气相色谱分析海水中的多环芳烃   总被引:22,自引:1,他引:21  
利用固相萃取搅拌棒(SBSE)萃取海水中的多环芳烃,然后用热解吸脱附-气相色谱分析。研究了萃取时间、添加NaCl浓度对萃取效率的影响。实验结果表明,SBSE方法对16种多环芳烃的萃取回收率分别在33.5%~122.4%之间;对标准样品的检出限为2.74-13.5ng/L;方法RSD为3.8%~13.1%。用此方法测定了大连海岸海水中的多环芳烃含量。  相似文献   

5.
采用溶胶—凝胶技术,加入自制的新化合物端羟基冠酸,成功地涂制了固相微萃取涂层;用半挥发性的有机污染物多环芳烃评价了涂层的基本性能,并对实际水样中的多环芳烃进行了分析。该方法的线性范围在0.1—10μg/L,检出限在0.001—0.03μg/L,8种多环芳烃化合物测定的相对标准偏差在2.05%一9.80%,回收率在85%以上。  相似文献   

6.
制备了一种二维的[Zn(benzotriazole)2]n配位聚合物,并经过XRD、SEM及元素分析法的表征,将其用于富集萃取环境水样中的6种重质多环芳烃,该配合物对于含多苯环的化合物显示出较强的吸附力。实验中分别对填料用量、淋洗剂、洗脱剂的种类及用量、穿透体积等参数进行考察,并将其与同等上样量及加标量的C18固相萃取小柱进行对比,建立了水样中6种多环芳烃的气相色谱-质谱联用检测方法。结果表明,使用200mg[Zn(benzotriazole)2]n配合物作为固相萃取填料,以10%甲醇为淋洗剂,0.5mL丙酮和5mL二氯甲烷作为洗脱剂,在上样体积为200mL、流速为4mL/min的条件下,6种多环芳烃均具有较高的回收率。荧蒽(Flan)、苯并(b)荧蒽(BbF)、苯并(g,h,i)芘(BghiP)的质量浓度在20~1000μg/L范围内,苯并(k)荧蒽(BkF)、苯并(a)芘(BaP)、茚并(1,2,3-Cd)芘(InP)在10~500μg/L范围内与峰面积呈良好线性关系,相关系数为0.9968~0.9993。方法的检出限为0.45~10.7ng/L,加标回收率为77%~112%,相对标准偏差为3.8%~8.5%。结果表明,该方法具有成本低、灵敏度高等特点,能够满足实际水样中6种多环芳烃的测定要求。  相似文献   

7.
超临界流体分级萃取正构烷烃和多环芳烃   总被引:10,自引:0,他引:10  
本工作用超临界CO2对环境模拟样品中的正构烷烃和多环芳烃的超临界分级萃取方法及超临界CO2的压力,温度和用量对分级效率的影响进行了详细的研究。结果表明,在低压、低温下(80MPa,50℃)能成功地分级萃取正构烷烃和多环芳烃,其C10~C18的萃取率为99.94%~59.28%,而多环芳烃基本未被萃取。当压力升至26.0MPa、温度升至80℃时,可有效地萃取多环芳烃,实现了正构烷烃和多环芳烃的有效分离  相似文献   

8.
加速溶剂萃取-气相色谱法测定土壤中16种多环芳烃   总被引:2,自引:0,他引:2  
利用加速溶剂萃取-气相色谱法测定土壤中16种多环芳烃的分析。研究了萃取时间、温度、压力、样品的粒度对萃取效率的影响及不同淋洗液在硅胶柱净化过程中对方法回收率的影响。实验结果表明,加速溶剂萃取方法对16种多环芳烃的萃取溶剂量小,萃取时间短萃取回收率分别在74%~95%之间;对标准样品的检出限为0.00004~0.02 mg/kg;方法RSD为4%~15%。用此方法测定了株洲土壤中的多环芳烃含量。  相似文献   

9.
本文以四丁基氯化铵和正辛醇制备的疏水性低共熔溶剂为绿色提取溶剂,结合高效液相色谱-荧光检测技术,构建了同时分析牛奶中芴、荧蒽、蒽、芘、■和苯并[a]芘6种多环芳烃类物质的新方法。系统地考察了各种萃取条件,包括萃取剂的种类、萃取时间、萃取温度、萃取剂用量以及盐的含量对牛奶中6种多环芳烃化合物提取效果的影响。结果表明,在优化的实验条件下,采用所制备的低共熔溶剂体系能较好地萃取上述6种多环芳烃化合物,三个水平的加标回收率为70.87%~100.45%,相对标准偏差为1.05%~8.95%,方法的检出限在0.03~0.3μg/kg之间。该方法快速、简便、环保,适用于牛奶中多环芳烃的测定。  相似文献   

10.
高效液相色谱法测定橡胶及其制品中16种多环芳烃   总被引:1,自引:0,他引:1  
经粉碎的橡胶样品用正已烷及丙酮(1+1)的混合溶剂萃取,所得萃取液蒸至近干后加入正己烷2 mL溶解残渣,将溶液经硅胶固相萃取柱分离并净化,吸附于柱上的多环芳烃用由正己烷及二氯甲烷(3+2)组成的淋洗液解吸,洗出液蒸至近干加入一定量的内标溶液使之溶解并用高效液相色谱法测定.选用LC-PAH色谱柱作固定相,用乙腈和水以不同比例混合的溶液作为流动相进行梯度淋洗,紫外检测器的测定波长为210 nm,以苝-d12作为内标进行定量测定,在优化的试验条件下16种多环芳烃可有效分离并测定.研究结果表明:16种多环芳烃的检出限(3S/N)、平均回收率及测定值的相对标准偏差(n=7)依次在0.05~0.10 mg·L-1,65.1%~101.7%及1.8%~7.3%之间.  相似文献   

11.
Solid phase extraction (SPE) with appropriate solid sorbents has been commonly used in the routine extraction of organic pollutants in water. The elution of analytes from the solid sorbents normally takes place by organic solvents under an applied vacuum. In this study, a microwave-assisted solvent elution technique was developed for the elution of analytes from C18 membrane disks during microwave irradiation from a microwave extraction system (MES). Several parameters, namely, elution solvent, elution temperature, duration of elution and the volume of solvent which may affect the elution efficiency of microwave-assisted solvent elution (MASE) technique towards organochlorine pesticides (OCPs), polychlorinated biphenyls (PCBs), polycyclic aromatic hydrocarbons (PAHs), phthalate esters (PAEs), organophosphorus pesticides (OPs), fungicides, herbicides and insecticides from the membrane disk were investigated. Good recoveries above 75% were obtained for most of the organic pollutants using the optimum SPE-MASE technique. The effect of sodium chloride and humic acid on the recoveries on the target analytes were also investigated.  相似文献   

12.
A solid-phase extraction (SPE) method using triacontyl bonded silica (C30) as sorbent was developed for the determination of 16 US Environmental Protection Agency polycyclic aromatic hydrocarbons (PAHs) in airborne particulate matters quantitatively by gas chromatography-mass spectrometry (GC-MS). Optimization experiments were conducted using spiked standard aqueous solution of PAHs and real airborne particulates samples aiming to obtain highest SPE recoveries and extraction efficiency. Factors were studied in SPE procedures including the concentration of organic modifier, flow rate of sample loading and elution solvents. The ultrasonication time and solvents were also investigated. Recoveries were in the range of 68-107% for standard PAHs aqueous solution and 61-116% for real spiked sample. Limits of detection (LODs) and limits of quantification (LOQs) with standard solution were in the range of 0.0070-0.21 microgL(-1) and 0.022-0.67 microgL(-1), respectively. The optimized method was successfully applied to the determination of 16 PAHs in real airborne particulate matters.  相似文献   

13.
SPE is a commonly applied technique for preconcentration of pesticides from water samples. Microwave‐assisted extraction (MAE) technique is the extraction applied for preconcentration of different compounds from solid samples. SPE coupled with MAE is capable of preconcentrating these compounds from water samples too. This investigation was aimed at improving the efficiency of atrazine, alachlor, and α‐cypermethrin pesticide extraction from the spiked water samples applying SPE followed by MAE. In this way, MAE served for elution of pesticides from C18‐extraction disks with solvent heated by microwave energy. Various elution conditions were tested for their effects on the extraction efficiency of the SPE–MAE combined technique. Several parameters, such as elution solvent volume (mL), elution temperature (°C), and duration of elution (min), affect the extraction efficiency of the SPE–MAE coupled system and need to be optimized for the selected pesticides. In order to develop a mathematical model, 15 experiments were performed in the central composite design. The equation was then used to predict recoveries of the pesticides under specific experimental conditions. Optimization of microwave extraction was accomplished using the genetic algorithm approach. Best results were achieved using 20 mL of ethanol at 60°C. Optimal hold time was 5 min and 24 s. The SPE–MAE combination was also compared with the conventional SPE extraction technique with elution of a nonpolar or a moderately polar compound with nonpolar solvents.  相似文献   

14.
A solid-phase extraction (SPE) method for sample clean-up, followed by reversed-phase high-performance liquid chromatography (HPLC) with fluorescence detection is reported for the determination of polycyclic aromatic hydrocarbons (PAHs) in edible oils. The effects of experimental variables, such as washing and elution solvents, sample solvent and drying time have been studied using C18 cartridges. Recoveries and selectivity using other sorbent materials (C8, C2, CH, PH and NH2) were also examined, with C18 being the best one. The recoveries ranged between 50 and 103% depending on the molecular mass of the PAH. The limits of quantitation were lower than 1 ng/g for most PAHs and good precision was achieved. The method was validated using certified reference materials.  相似文献   

15.
The coupling of solid-phase extraction (SPE) using bamboo charcoal (BC) as an adsorbent with a monolithic column-high performance liquid chromatography (MC-HPLC) method was developed for the high-efficiency enrichment and rapid determination of 16 polycyclic aromatic hydrocarbons (PAHs) in water. Key influence factors, such as the type and the volume of the elution solvent, and the flow rate and the volume of the sample loading, were optimized to obtain a high SPE recovery and extraction efficiency. BC as an SPE adsorbent presented a high extraction efficiency due to its large specific surface area and high adsorption capacity; MC as an HPLC column accelerated the separation within 8 min because of its high porosity, fast mass transfer, and low-pressure resistance. The calibration curves for the PAHs extracted were linear in the range of 0.2-15 μg/L, with the correlation coefficients (r(2)) between 0.9970-0.9999. This method attained good precisions (relative standard deviation, RSD) from 3.5 to 10.9% for the standard PAHs I aqueous solutions at 5 μg/L; the method recoveries ranged in 52.6-121.6% for real spiked river water samples with 0.4 and 4 μg/L. The limits of detection (LODs, S/N = 3) of the method were determined from 11 and 87 ng/L. The developed method was demonstrated to be applicable for the rapid and sensitive determination of 16 PAHs in real environmental water samples.  相似文献   

16.
Triacontyl bonded silica (C(30)) material was applied as solid-phase extraction (SPE) sorbent and an SPE-LC-MS method was established for the determination of eight estrogens and their metabolites in water samples. Compared to commercial C(18) SPE cartridge, the performance of C(30) was evaluated in various important SPE conditions, such as sorbent mass, elution solvent and its volume, loading flow rate, and sample loading volume. The results showed a superior performance of C(30)-C(18) by the shorter treatment time and fewer required elution solvent. In the optimum conditions, the results showed good recoveries (80.5-109.4%), excellent linear relationships (0.02-1 ng/mL, except 2-MeO-E(2)), high precisions (lower than 10.0% RSD for both low and high spiked concentration), and low LODs (1-16 ng/L). Method validation using C(30) packed cartridge was also testified with spiked real water samples, including tap water and river water. Satisfy results demonstrated the feasibility of C(30) SPE to the analysis for real environmental waters.  相似文献   

17.
The graphene functionalized with (3‐aminopropyl) triethoxysilane was synthesized by a simple hydrothermal reaction and applied as SPE sorbents to extract trace polycyclic aromatic hydrocarbons (PAHs) from environmental water samples. These sorbents possess high adsorption capacity and extraction efficiency due to strong adsorption ability of carbon materials and large specific surface area of nanoparticles, and only 10 mg of sorbents are required to extract PAHs from 100 mL water samples. Several condition parameters, such as eluent and its volume, adsorbent amount, sample volume, sample pH, and sample flow rate, were optimized to achieve good sensitivity and precision. Under the optimized extraction conditions, the method showed good linearity in the range of 1–100 μg/L, repeatability of the extraction (the RSDs were between 1.8 and 2.9%, n = 6), and satisfactory detection limits of 0.029–0.1 μg/L. The recoveries of PAHs spiked in environmental water samples ranged from 84.6 to 109.5%. All these results demonstrated that this new SPE technique was a viable alternative to conventional enrichment techniques for the extraction and analysis of PAHs in complex samples.  相似文献   

18.
A solid-phase extraction (SPE) using graphene as adsorbent coupled with capillary zone electrophoresis method was developed for the determination of four sulfonamide residues (sulfadimidine, sulfadimethoxine, sulfathiazole and sulfadiazine) in meat sample. Several condition parameters, such as elution solvents and volumes, sample pH and sample volume were optimized to obtain high SPE recoveries and extraction efficiency. Intra-day precisions of sulfonamides were in the range of 2.5–2.6 % and the inter-day precisions of sulfonamides were in the range of 2.6–3.4 %. Recoveries were 60.9–66.6 % for sulfadiazine and 86.1–111.4 % for other three sulfonamides in spiked meat sample. The developed method was successfully applied for the determination of sulfonamides in meat samples.  相似文献   

19.
A green and novel deep eutectic solvent modified graphene was prepared and used as a neutral adsorbent for the rapid determination of sulfamerazine in a river water sample by pipette‐tip solid‐phase extraction. Compared with conventional graphene, deep eutectic solvent modified graphene can change the surface of graphene with wrinkled structure and higher selective extraction ability. The properties of deep eutectic solvent modified graphene and graphene were characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, and thermogravimetric analysis. Static adsorption showed deep eutectic solvent modified graphene had a higher adsorption ability (18.62 mg/g) than graphene. Under the optimum conditions, factors such as kinds of washing solvents and elution solvents and volume of elution solvent were evaluated. The limits of detection and quantification were 0.01 and 0.03 μg/mL, respectively. The method recoveries of sulfamerazine were in the range of 91.01–96.82% with associated intraday relative standard deviations ranging from 1.63 to 3.46% and interday relative standard deviations ranging from 0.68 to 3.84%. Deep eutectic solvent modified graphene showed satisfactory results (recovery was 95.38%) and potential for rapid purification of sulfamerazine in river water sample in combination with the pipette‐tip solid‐phase extraction method.  相似文献   

20.
A solid-phase extraction (SPE) using multi-walled carbon nanotubes (MWCNTs) as adsorbent coupled with gas chromatography–mass spectrometry (GC–MS) method was developed for the determination of 16 polycyclic aromatic hydrocarbons (PAHs) in environmental water samples. Several condition parameters, such as extraction adsorbents, elution solvents and volumes, and sample loading flow rate and volume were optimized to obtain high SPE recoveries and extraction efficiency. 150 mg MWCNTs as sorbent presented high extraction efficiency of 16 PAHs due to the large specific surface area and high adsorption capacity of MWCNTs compared with the commercial C18 column (250 mg/2 mL). The calibration curves of 16 PAHs extracted were linear in the range of 20–5000 ng L−1, with the correlation coefficients (r2) between 0.9848 and 0.9991. The method attained good precisions (relative standard deviation, RSD) from 1.2% to 12.1% for standard PAHs aqueous solutions; method recoveries ranged in 76.0–125.5%, 74.5–127.0%, and 70.0–122.0% for real spiked samples from river water, tap water and seawater, respectively. Limits of detection (LODs, S/N = 3) of the method were determined from 2.0 to 8.5 ng L−1. The optimized method was successfully applied to the determination of 16 PAHs in real environmental water samples.  相似文献   

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